The aroma compounds of ayran were isolated using solvent-assisted flavor evaporation (SAFE) resulting in a more representative extract of ayran odor compared to liquid-liquid extraction (LLE), solid-phase extraction (SPE), and simultaneous distillation-extraction (SDE). The aromatic extract was subjected to sensory analysis and identified and quantified by gas chromatography-mass spectrometry (GC-MS). A total of 19 volatile compounds were detected that included alcohols, aldehyde, acids, esters, ketones, and terpenes. However, the compounds present at the highest concentrations were ethyl lactate, ethanol, 2,3-butanediol, acetoin, and acetic acid. The key odorants for the ayran drinks were detected using aroma extract dilution analysis (AEDA) and GC-MS-olfactometry (GC-MS-O). A total of 14 aroma-active compounds were determined for the first time. The flavor dilution (FD) factors ranged between 4 and 512 while their odor activity values (OAVs) were from 1.35 to 1126.99. Ethyl lactate (FD of 512 whey/creamy), 2-methylbutanal (FD of 512, fruity), acetoin (FD of 256, buttery creamy), and butanoic acid (FD of 256, cheesy-sweet) were the strongest aroma-active components of the Ayran drink.